in acetone refluxed in acetone for 5 h under N2 atmosphere, filtration of excess Fe(CO)5, solvent removed in vac.; dissolved in CH2Cl2, chromd. on silica gel, eluent petroleum ether/chloroform (4:1);
参考文献
Aime, Silvio; Milone, Luciano; Osella, Domenico; Tiripicchio, Antonio; Manotti Lanfredi, Anna Maria
Inorganic Chemistry, 1982 , vol. 21, p. 501 - 505
in acetone refluxed in acetone for 5 h under N2 atmosphere, filtration of excess Fe(CO)5 solvent removed in vac., further products; dissolved in chloroform and chromd. on silica gel, eluent petroleum ether and chloroform, elem. anal.;
参考文献
Aime, Silvio; Milone, Luciano; Osella, Domenico; Tiripicchio, Antonio; Manotti Lanfredi, Anna Maria
Inorganic Chemistry, 1982 , vol. 21, p. 501 - 505
in benzene Ar-atmosphere; stirring Os-complex with excess of Fe-complex (room temp., 2 h), refluxing for 10 h; filtration, evapn., chromy. (SiO2, hexane);
参考文献
Maksakov; Kirin; Virovets; Podberezskaya; Semyannikov
Journal of Organometallic Chemistry, 1997 , vol. 543, # 1-2 p. 57 - 62
→
反应条件
air in methanol; water (N2); using Schlenk techniques; dissolving of (NEt3H)(HFe3(CO)11) in soln. of KOH in MeOH; stirring overnight; monitoring by IR; bubbling streamof air; removal solvent under reduced pressure, dissolving in H2O; addn . of CsCl; pptn., addn. 20percent H2SO4; pptn., extn. with toluene, elimination Fe3(CO)12; extn. with CH2Cl2 and then with THF; layering of hexane; crystn., mechanical sepn.; elem. anal.;
in water; pentane Ar-atmosphere; addn. of excess of Fe-complex suspn. (in pentane) to Os-complex suspn. (in H2O), stirring for 6 h; filtration, addn. of 70percent H3PO4 and ether; in air; sepn. of ether layer, drying (MgSO4), chromy. (SiO2, hexane);
参考文献
Maksakov; Kirin; Virovets; Podberezskaya; Semyannikov
Journal of Organometallic Chemistry, 1997 , vol. 543, # 1-2 p. 57 - 62
in diethyl ether under N2, educts (2.2:5.5 ratio), at room. temp. for 18 h; solvent evapd., residue treated with hexane, cooled to -20°C product crystd. filtered, rest of products sepd. by chromy.(Al2O3, hexane/ether);
in petroleum ether refluxed in acetone for 5 h under N2 atmosphere, filtration of excess Fe(CO)5 solvent removed in vac.; dissolved in chloroform and chromd. on silica gel, eluent petroleum ether and chloroform, not sepd. products;
参考文献
Aime, Silvio; Milone, Luciano; Osella, Domenico; Tiripicchio, Antonio; Manotti Lanfredi, Anna Maria
Inorganic Chemistry, 1982 , vol. 21, p. 501 - 505
Nametkin,N.S. et al.
Bulletin of the Academy of Sciences of the USSR, Division of Chemical Science (English Translation), 1976 , vol. 25, p. 1595
Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, 1976 , vol. 25, p. 1678